Large glassy beads

ABSTRACT

The present invention relates to a particulate composition in the form of a large spherical glassy bead having a cross-sectional diameter greater than 5 mm. The bead comprises an encapsulating carrier composition essentially made of fibrous materials, which are both sugarless and non-cariogenic and an encapsulant, such as a flavor material.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. application Ser. No.11/484,450 filed Jul. 10, 2006, now U.S. Pat. No. 8,227,014, which is acontinuation of International Application No. PCT/IB2005/000145 filedJan. 20, 2005, the entire content of each of which is expresslyincorporated herein by reference thereto.

TECHNICAL FIELD

The present invention relates to the field of encapsulation. It concernsmore particularly a novel delivery system capable of releasing an activeingredient such as a flavor and wherein a novel encapsulating carriercomposition which is essentially made of fibrous materials, and moreparticularly of a combination of two particular fibrous polysaccharidesenables the preparation, through an extrusion process, of large glassybeads. The solid particulate composition of the invention can constitutea ready-to-consume end product intended for the confectionery area, orbe used as a delivery system for a flavor or another active ingredient,when added to a consumer product, for example when added to an ediblecomposition such as a foodstuff or beverage.

BACKGROUND ART

The literature discloses many ways of providing active ingredients in anencapsulated form. The encapsulation of active ingredients has variousobjectives, the main being, on the one hand, to protect labile orvolatile ingredients from a degradation or any adverse interaction withan external element, and on the other hand to control the release of theencapsulated active ingredient and provide an efficient release onlywhen desired, depending on the application.

Encapsulation methods and encapsulating matrix compositions areparameters which can be varied and are chosen as a function of thepurpose for which a delivery system is designed. They are the object ofmany patents or patent applications.

Regarding encapsulation methods, extrusion has been widely described inthe prior art, particularly in the patent literature. This methodtypically relies on the use of carbohydrate matrix materials which areheated to a molten state and combined with an active ingredient, beforeextruding and quenching the extruded mass to form a glass which protectssaid ingredient. Typical products issued from this method and used inthe flavor industry are dry, granular delivery systems in which theactive ingredient is a flavor uniformly distributed as dropletsthroughout a carbohydrate glass. One significant example of the priorart disclosures in this field is U.S. Pat. No. 3,704,137 which describesan essential oil composition formed by mixing an oil with anantioxidant, separately mixing water, sucrose and hydrolysed cerealsolids with dextrose equivalent (DE) below 20, emulsifying the twomixtures together, extruding the resulting mixture in the form of rodsinto a solvent, removing the excess of solvent and finally adding ananti-caking agent. Another pertinent example is that described in U.S.Pat. Nos. 4,610,890 and 4,707,367 which disclose a process for forming astable, melt based and extruded, solid, essential oil flavorcomposition, as well as a product of this process. The melt to beextruded consists, in this particular case, in a matrix formed of anaqueous mixture of a sugar and a starch hydrolysate together with aselected emulsifier, said aqueous mixture being further blended with aselected quantity of essential oil flavor. More recently, U.S. Pat. No.6,707,771 has described a novel extrusion process wherein the extrudedmass is chopped as it exits the die and when it is in a plastic state.This process avoids any drying step following extrusion. Theabove-mentioned patents are merely illustrative of the considerablevolume of patent literature related to extrusion techniques.

Carrier materials described as being suitable for extrusion processesare also numerous. The most useful ingredients are long chaincarbohydrates typically including starches, hydrogenated starchhydrolysates, modified starches and gums, in combination with or asalternative of low molecular weight carbohydrates such as mono- ordisaccharides, maltodextrins having a dextrose equivalent (DE) in therange of about 4 to 20, and corn syrup solids or polydextrose having adextrose equivalent in the range of about 21 to 97.

Now, the present invention relates to a novel encapsulating carriercomposition essentially made of fibrous polysaccharides and moreparticularly made of soluble dietary fibres. Dietary fibres are commonlydefined as polysaccharides which are resistant to the endogenous enzymesof man, i.e., that they are not digested by the endogenous secretions ofthe human digestive tract. They are divided into water-insoluble andwater-soluble fibres. Water-soluble fibres have been widely described inthe prior art because of their known health benefits, as ingredientsused in food products, partly because they reduce the glycemic responseto food and make thus food products which contain soluble fibresparticularly suitable for diabetics. This prior art describes the use ofwater-soluble fibres as such in ready-to-consume products, but not aspotential encapsulating materials.

On the other hand, soluble and insoluble fibres have also been disclosedas being potentially useful to be added in minor amounts toencapsulating compositions to control the release of the encapsulant(PCT publication WO 99/48372).

U.S. Pat. No. 6,468,568 discloses the encapsulation of a mineral such ascalcium or a vitamin, in a double encapsulation system containing afibre material. The active ingredient is firstly surrounded by an edibleoil and then encapsulated in a glassy matrix composition including anoligosaccharide, which may be inulin. Inulin is a clean, dried fibrousmaterial which is separated by extraction from, for example, chicory,onions or Jerusalem artichokes and other common plant sources. It is theonly totally fibrous material mentioned in this document among otheroligosaccharides. All the other oligosaccharide materials suitable forthe purpose disclosed herein include sugars. The encapsulation methoddescribed in this document is extrusion and allows to obtain a productwhich is non-rubbery and readily grindable into fine particulatecompositions or powders ready for incorporation into or onto foodcompositions. The glassy matrix compositions described can be extrudedthrough extrusion dies having aperture diameters of from about 0.10 mmto about 5 mm. The diameter of the extrudate rope and product may belarger than the diameter of the die apertures due to deformation orswelling as the composition exits the die. The increase in diameter uponexiting the die may occur without substantial development of anexpanded, puffed, foamy, or cellular structure. According to the presentinvention, we have been able to realise a novel encapsulating carriercomposition which, in addition to the fact that it consists essentiallyof fibrous materials and thus presents advantageous properties such asbeing sugar-free and non-cariogenic, enables the preparation of aparticulate composition with a larger size than disclosed in the priorart, namely with a cross-sectional diameter of at least 3, preferably atleast 5 mm and up to 15 mm. The products of the invention are thereforesuitable either for direct consumption in applications in the sweet andsavoury confectionary area and bakery area where they providealternative products to known gelatine type candies, or small compressedtablets, or for an use as an efficient delivery system when added to anedible composition such as a foodstuff or beverage.

DISCLOSURE OF THE INVENTION

The present invention relates to a novel particulate composition in theform of a large glassy bead made of an essentially fibrous carriercomposition. More particularly, a first object of the invention is aparticulate composition in the form of an extruded, glassy bead,comprising a fibrous, carrier composition encapsulating an activeingredient, wherein the bead has a cross-section diameter comprisedbetween 3 mm and 15 mm, preferably between 5 mm and 15 mm, morepreferably between 6 mm and 15 mm and is preferably spherical. The sizeof the bead of the invention is linked to its characteristic carriercomposition, which is essentially made of water-soluble fibrousmaterials, and which comprises more particularly one long-chainwater-soluble fibrous polysaccharide and another fibrous material oflower molecular weight. The specific choice of water-soluble fibresconstituting the carrier composition of the product of the invention anddefined below by their respective average molecular weights and degreesof polymerisation allows, through an extrusion process, to provide asignificant relaxation phenomenon of the polymeric carriers at the endof the die of the extruder, leading to, for example, spherical beadswith a diameter larger than 3, preferably larger than 4, more preferablylarger than 5 mm and even more preferably larger than 6 mm. On the otherhand, the nature of the fibrous materials advantageously imparts to thefinal product qualities such as non-cariogenicity and sugarless nature,which render it particularly useful for the preparation of specificproducts of the sweet and savoury confectionery area and bakery area, orfor an use as a traditional delivery system for flavor or other activeingredients, when added to a ready-to-consume end product.

End consumer products are also objects of the present invention. Inparticular for the flavor industry, products such as chewy sweets, gummycandies, hard boiled candies, cookies, cakes and baked applications ingeneral and cereal bars, chocolate bars and back-pack dairy canadvantageously use the particulate compositions of the invention asflavoring ingredients.

Savoury goods can also be flavored with the beads of the invention, forinstance noodles or soups. The size of the delivery systems gives anappreciated visual effect in the final application, while providing anefficient protection of the volatile and labile ingredient encapsulatedand a controlled release of the latter, i.e. a release occurring only atthe time of consumption of the end product. In other words, the productsof the invention are used in applications both for their qualities asefficient delivery systems and for their visual aspect which differsfrom usually used encapsulated systems.

Other benefits and advantages of the product of the invention willbecome apparent through the detailed description and the examples givenbelow.

The particulate composition of the invention is in the form of anextruded, glassy bead, comprising a fibrous carrier compositionencapsulating an active ingredient, wherein the bead has a cross-sectiondiameter comprised between 3 mm and 15 mm, preferably between 5 mm and15 mm, more preferably between 6 mm and 15 mm and the carriercomposition comprises from 1 to 70% by weight of a first water-solublefibrous polysaccharide having an average molecular weight higher than10,000 Dalton (Da) and an average degree of polymerisation higher than60, and from 30 to 99% of a second water-soluble fibrous polysaccharidehaving an average molecular weight below 10,000 Da and an average degreeof polymerisation below 60, percentages being given by weight relativeto the total weight of the carrier composition.

The term water-soluble polysaccharide means that the polysaccharide isat least 50% soluble according to the method described by L. Prosky etal., J. Assoc. Off. Anal. Chem. 71, 1017-1023 (1988). As was mentionedbefore, the term fibre or fibrous polysaccharide refers to the fact thatthe polysaccharide cannot be digested or hydrolysed by the endogenoussecretions of the human digestive tract. Accordingly, the termnon-fibrous polysaccharide means that the polysaccharide can be digestedby the endoenuous secretions of the human digestive tract.

The particulate composition comprises a specific encapsulating carrierwhich is essentially made of fibres. The term “carrier”, also referredto as “matrix”, is commonly used in the encapsulation art to designatethe encapsulating composition in a delivery system, i.e. the compositionwherein the active ingredient to be protected is entrapped. Whilefibrous materials have sometimes been mentioned as being possibly addedto an encapsulating composition, in particular to control the release ofthe encapsulant, a specific combination of fibrous materials allowingthe preparation by extrusion of beads of the size defined in the presentinvention has never been described. More particularly, the only documentfrom the prior art which, to our knowledge, encompasses the possibilityof having a carrier entirely made of a fibre (such embodiment beinghowever non exemplified in U.S. Pat. No. 6,468,568), only allows toprepare a particulate composition of a common size for extrudedproducts, i.e. smaller than 5 mm. Now, in the present invention, we havebeen able to establish that a specific combination of water-solublefibrous materials defined by means of average molecular weights anddegrees of polymerisation, allows to prepare a melt that can be extrudedand, thanks to a relaxation phenomenon of the polymeric polymers at theexit of the extruder, to prepare large beads, in particular sphericalbeads with a cross-sectional diameter higher than 3 mm, preferablyhigher than 4 mm, more preferably higher than 5 mm. Sugars such as mono-and disaccharides commonly used in large proportions in carriercompositions to be extruded prevent significant polymer relaxation. Thecarrier composition encapsulating the active ingredient in the presentinvention is advantageously free of this type of compounds and can thusbe described as being sugarless.

The first water-soluble polysaccharide present in the carrier orencapsulating composition of the product of the invention is a solublefibre having an average molecular weight higher than 10,000 Dalton (Da)and an average degree of polymerisation higher than 60. This long-chainpolymer is present in proportions varying between 1 and 70% by weight,relative to the total weight of the carrier composition, preferablybetween 2 and 50%, more preferably between 8 and 20% by weight, forexample between 2 and 20% by weight. In a particular embodiment of theinvention, it is chosen from the group consisting of konjac mannan,xanthan, gum Arabic, guar gum, pectin, locus bean gum, soluble soyabeanpolysaccharide and beta-glucan.

The second water-soluble polysaccharide present in the carriercomposition of the bead is a fibre with a smaller molecular weight. Inparticular, the latter has an average molecular weight below 10,000 Daand an average polymerisation degree below 60. Typically, it is adextrin. It is comprised in proportions varying between 20 and 99%, forexample, between 30 and 99%, by weight and preferably between 50 and98%, for example between 80 and 98% by weight relative to the totalweight of the carrier composition. A particularly suitable dextrin forthe invention has a Chemical Abstract Registry Number of 9004-53-9. Thismaterial is commercially available from Roquette Freres as Nutriose FB®,marketed as a new soluble dietary fibre offering good digestivetolerance, acid and heat resistance, and bulking effect for sugar-freeproducts. To the best of our knowledge, no use of this material as anadvantageous encapsulating material for the preparation of an extrudeddelivery system has been described up to now.

Preferably, the carrier composition comprises less than 20wt. % ofnon-fibrous polysaccharides, more preferably less than 10 wt. %, evenmore preferably less than 5 wt. % of non-fibrous polysaccharides. Mostpreferably, it is free of non-fibrous polysaccharides.

Preferably, the first and/or the second polysaccharide arenon-cariogenic. More preferably, both polysaccharides arenon-cariogenic.

In an embodiment of the present invention, the carrier composition issugarless and/or non-cariogenic.

Preferably, the carrier composition has a low glycemic index, that is aglycemic index below 55. More preferably, the glycemic index of thecarrier composition is below 40, most preferably it is below 25.

In addition to these essential main components of the encapsulatingmaterial, the carrier may comprise a plasticizer, typically inproportions varying between 1 and 10% by weight relative to the totalweigh of the particulate composition. Plasticizers commonly used inextrusion techniques suit the invention and are well known to a personskilled in the art. They include, while not being limited to, water,propylene glycol, isomalt, glycerol, ethylene glycol, dipropyleneglycol, triacetine, organic acids and mixtures thereof.

The carrier composition can also comprise optional ingredients, such ascolorants or emulsifiers. Typical examples of emulsifiers includelecithin, citric esters of fatty acids, but other suitable emulsifiersare cited in reference texts such as Food emulsifiers and theirapplications, 1997, edited by G. L. Hasenhuettl and R. W. Hartel. A moredetailed description of these ingredients is not necessary in thepresent case as these ingredients are commonly used during the extrusionof any carrier composition and are well known by a skilled person in theart.

The carrier composition of the invention encapsulates an activeingredient preferably comprised in proportions varying between 0.01 and15% by weight, more preferably between 0.05 and 3% by weight, relativeto the total weight of the particulate composition. The activeingredient protected in the delivery system of the invention can be asvaried as flavors, fragrances, vitamins, drugs or coloring materials,for example. In an embodiment of the present invention, the activeingredient is selected from the group consisting of a flavor, afragrance, a vitamin, a drug, a colorant, a nutraceutical, a whiteningagent, an antibacterial agent, and a mixture comprising at least two ofthese. The active ingredient may be a volatile or a labile componentwhich may be in liquid or solid form. Preferably, the active ingredientis hydrophobic. For example, it is a flavor or fragrance ingredient orcomposition. The terms “flavor or fragrance ingredient or composition”as used herein are deemed to define a variety of flavor and fragrancematerials of both natural and synthetic origin. They include singlecompounds and mixture. Specific examples of such components may be foundin the current literature, e.g. in Perfume and Flavour Chemicals by S.Arctander, 1969, Montclair N.J. (USA); Fernaroli's Handbook of FlavourIngredients, 1975, CRC Press or Synthetic Food Adjuncts, 1947, by M. B.Jacobs, van Nostrand Co., Inc and are well known to the person skilledin the art of perfuming, flavoring and/or aromatising consumer products,i.e. of imparting an odor and/or a flavor or taste to a consumer producttraditionally perfumed or flavored, or of modifying the odor or taste ofsaid consumer products.

Natural extracts can also be encapsulated into the system of theinvention ; these include e.g. citrus extracts such as lemon, orange,lime, grapefruit or mandarin oils, or coffee, tea, cocoa, mint, vanillaor essential oils of herbs and spices, amongst other.

A nutraceutical may also be an active ingredient of the particulatecomposition of the invention. Nutraceuticals are compounds, ingredientsor a dietary supplement or a food that has health and medical benefits,including the prevention and treatment of disease. Nutraceuticalsinclude antioxydants, amino acids and proteins, botanicals, probiotics,nutritional fats (for example, polyunsaturated fatty acids PUFAs), soy,vitamins, and minerals. For example, the nutraceutical may be DHA, whichhas the beneficial effect of reducing the occurrence of cardio-vasculardiseases.

Examples for whitening agents are baking soda, hydrogen peroxide andpapain. Examples of antibacterials are triclosan, pyrophosphate,propolis and natural essential oils. The active ingredient may also bean ingredient for treating or preventing bad breath or breath malodor,for example green tea or parsley oil, or an antiplaque agent, forexample tetra and bi-natrium, tetra and bi-potassium.

Furthermore, the active ingredient may be a mixture comprising differentingredients, for example it may be a mixture comprising differentflavors. In an embodiment of the present invention, the activeingredient is a mixture comprising a flavor and a nutraceutical.

A process for the preparation of the particulate composition of theinvention is also an object of the present invention. The processcomprises the steps of combining and blending the active ingredient tobe encapsulated with a carrier composition comprising from 1 to 70% byweight of a first water-soluble fibrous polysaccharide having an averagemolecular weight higher than 10,000 Da and an average degree ofpolymerisation higher than 60, and from 30 to 99% of a secondwater-soluble fibrous polysaccharide having an average molecular weightbelow 10,000 Da and an average degree of polymerisation below 60,percentages being given by weight relative to the total weight of thecarrier ; heating said blend within a screw extruder to a temperaturecomprised between 80° C. and 120° C. to form a molten mass ; thenextruding the molten mass through a die having a die hole diametercomprised between 4 and 12 mm ; and cutting the material obtained as itexits the die. Typical conditions for this process are those commonlyused in the art and are well know by a skilled person, they thus do notneed a more detailed description here. Specific conditions will beexemplified below.

The apparatus suitable for carrying out the process of the invention isa single or twin screw extruder. It allows to continuously mix theingredients and subsequently extruding the composition through anextrusion die plate. The extrusion dies suitable for the invention havehole diameters of from about 2 mm to about 12 mm, preferably from about3 mm to about 10 mm, for example from about 4 mm to about 12 mm,generally less than 7 mm. The extruded particulate composition, due toits specific carrier composition, is subjected to a significantrelaxation phenomenon at the end of the die, which allows to produce anextruded rope having a cross-sectional diameter larger than 3mm, 4mm,5mm, or 6mm, for example, and which can be as large as about 15 mm. Theprocess of the invention thus allows to prepare beads, preferably with aspherical shape, presenting such cross-sectional diameter, which was notpossible up to now. In fact, spherical particles prepared by extrusionhave already been described, but they had much smaller sizes. Thespherical shape of the beads should not be intended as limiting theinvention. In fact, by varying the die shape and the moment when theextruded rope is cut, other bead shapes can be obtained by the processof the invention, for instance bean-type shapes.

The product obtained by the process of the invention is a solidparticulate composition, in a glassy state. More particularly the beadof the invention has a glass transition temperature, Tg, above roomtemperature, namely above a temperature usually comprised between 18 and25° C. The product is thus in a brittle form, which gives it a so-called“crunchy” character when consumed or used.

The particulate composition of the invention can be used in many fieldsof application. First of all, in the flavor industry, the large beadshere-described can be used in many ready-to-consume products, as aflavoring ingredient, or even as constituting an end-product itself. Infact, the carrier composition has, as a consequence of its specificfibrous composition, the properties of being non-cariogenic andsugarless or even sugar-free. By non-cariogenic, one designates aproduct which shows lower acidification by bacteria from the mouth thanclassical sugar such as saccharose, glucose and fructose. Theseproperties render the carrier composition particularly useful inapplications in the food area where it is desired to havetooth-friendly, non-cariogenic and sugarless or even sugar-freeproducts, for instance for products intended to the confectionery field.In this area and thanks to its size, the particulate composition of theinvention constitutes an advantageous alternative to existing edibledelivery systems such as gelatine type candies, small compressed tabletsor coated compressed tablets. On the other hand, if it is desired tomodify the release condition of the active ingredient, the particulatecomposition of the invention can also be subjected to a coating, forexample by means of a wax. The coating may then be flavored itself witha flavor different from the encapsulated one, thus providing a “dualrelease”, i.e. the perception of various flavor tonalities duringconsumption by sucking.

On the other hand, large beads of the invention can also be used as aflavor delivery system, the main advantage being its size and burstingeffect in application, in addition to the visual appeal. The system isadded to a composition in order to improve, enhance or modify theorganoleptic properties of a great variety of edible end products.

Thus, the method of using the specific combination of fibrous materialsas a novel carrier composition for the preparation of a delivery systemis another object of this invention, as carriers known and used up tonow, did not allow to produce by extrusion a product of the presentquality and with the claimed dimensions and shapes.

Typical products possibly flavored by means of the beads of theinvention include, but are not limited to a baked product, for example acake or a cookie, a hard-boiled candy, a gummy candy, a chewy sweet, achewing gum, a cereal bar, a soup, noodles or savoury snacks. Of these,a hard boiled candy having a spherical form is preferred.

When the active ingredient encapsulated in the particulate compositionhere-described is a perfume, the beads thus prepared are suitable forapplications for instance in functional perfumery, for products such asbath salts, shower or bath gels, shampoos, conditioners or otherhair-care products, deodorants and antiperspirants, as well as airfresheners, detergents and fabric softeners.

The concentrations in which the extruded beads can be incorporated insuch consumer products vary in a wide range of values, which aredependent on the nature of the product to be flavored or perfumed, or towhich is it desired to add a vitamin or a dye. Typical concentrations,to be taken strictly by way of example, are comprised in the range ofvalues as wide as from a few ppm to 5 or even 10% of the weight of thecomposition or finished consumer product into which they are included.

EXAMPLES

The invention will now be illustrated by way of the following examplesbut is not limited to these examples. Temperatures are given in degreescentigrade and abbreviations have the meaning common in the art.

Examples 1-4: Particulate Composition According to the Invention withDifferent Flavors Example 1 Particulate Composition According to thePresent Invention With Menthol Flavor and Use Thereof as a Sugarless,Non-Cariogenic Candy

A particulate composition was prepared with the following ingredients:

Ingredients weight (g) NUTRIOSE FB ®¹⁾ 838.00 Gum Arabic 129.90 MentholNat²⁾ 12.01 Acesulfam K 3.50 Aspartame 6.54 Dye 0.05 Emulsifier 10.00Total 1000.00 ¹⁾origin: Roquette Freres, France ²⁾ref number 957789;origin: Firmenich SA, Geneva, Switzerland

The ingredients mentioned above were mixed together so as to produce adry blend. This powder blend was then extruded with 4% water added, at athroughput of 6 kg/h through a 4 mm die hole using a twin screw extruderequipped with a cutterknife allowing to chop the melt at the die exitwhile it is still plastic. At the low water content needed to guaranteea glass transition above 40° C. at constant sample composition, thetemperature of the melt in the front plate was of 100° C. and theplastic pressure in the extruder was preferably kept higher than 3×10⁵Pa and below 30×10⁵ Pa.

There were obtained spherical beads with a cross-sectional diameter of 6mm, and a glass transition temperature of 56° C.

The product constitute a ready-to-consume non-cariogenic, and sugar-freecrunchy candy having a menthol flavor.

Example 2 Particulate Composition With Lemon Flavor

A particulate composition was prepared with the following ingredients:

Ingredients weight (g) NUTRIOSE FB ®¹⁾ 807.00 Gum Arabic 130.34 Lemonflavor²⁾ 7.00 Acid citric 14.98 Acesulfam K 3.43 Aspartame 6.55 Yellowdye 0.70 Emulsifier 10.00 Lemon juice³⁾ 20.00 Total 1000.00 ¹⁾origin:Roquette Freres, France ²⁾ref number 505594 A; origin: Firmenich SA,Geneva, Switzerland ³⁾ref number 925714; origin: Firmenich SA, Geneva,Switzerland

The ingredients mentioned above were mixed together so as to produce adry blend. This powder blend was then extruded with 4% water added, at athroughput of 6 kg/h through a 4 mm die hole using a twin screw extruderequipped with a cutterknife allowing to chop the melt at the die exitwhile it is still plastic. At the low water content needed to guaranteea glass transition above 40° at constant sample composition, thetemperature of the melt in the front plate was of 92° and the plasticpressure in the extruder was preferably kept higher than 3×10⁵ Pa andbelow 30×10⁵ Pa.

There were obtained spherical beads with a cross-sectional diameter of 6mm, and a glass transition temperature of 50°.

Example 3 Chocolate Flavored Particulate Composition of to the PresentInvention

A particulate composition was prepared with the following ingredients:

Ingredients weight (g) NUTRIOSE FB ®¹⁾ 756.00 Gum Arabic 129.95 Vanillin7.05 Acesulfam K 3.53 Aspartame 6.47 Emulsifier 10.00 Chocolate flavor²⁾50.00 Caramel powder colorant 37.00 Total 1000.00 ¹⁾origin: RoquetteFreres, France ²⁾ref number 505899 T; origin: Firmenich SA, Geneva,Switzerland

The ingredients mentioned above were mixed together so as to produce adry blend. This powder blend was then extruded with 3% water added at athroughput of 6 kg/h through a 4 mm die hole using a twin screw extruderequipped with a cutterknife allowing to chop the melt at the die exitwhile it is still plastic. At the low water content needed to guaranteea glass transition above 40° C. at constant sample composition, thetemperature of the melt in the front plate was of 90° C. and the plasticpressure in the extruder was preferably kept higher than 3×10⁵ Pa andbelow 30×10⁵ Pa.

There were obtained spherical beads with a cross-sectional diameter of 6mm, and a glass transition temperature of 44° C.

Example 4 Tutti Frutti Flavored Particulate Composition

A particulate composition was prepared with the following ingredients:

Ingredients weight (g) NUTRILOSE FB ®¹⁾ 839.99 Gum Arabic 130.00 Tuttifrutti flavor composition²⁾ 5.00 Citric acid 5.00 Acesulfam K 3.50Aspartame 6.50 Emulsifier 10.00 Dye 0.01 Total 1000.00 ¹⁾origin:Roquette Freres, France ²⁾ref number 51880 A; origin: Firmenich SA,Geneva, Switzerland

Following the same procedure as given in Example 3, there were obtainedspherical beads with a cross-sectional diameter of 6 mm, and a glasstransition temperature of 44° C.

Examples 5-8: Food Applications Comprising the Particulate Compositionof the Invention Example 5 Baked Cake Flavored With a ParticulateComposition of the Invention

A cake was prepared with the following ingredients:

Ingredients weight (g) Part A Flour 75.00 Beatreme SE¹⁾ 75.00 Granulatedsucrose 57.50 Baking powder 4.50 Corn starch 2.50 Salt 0.50 Part BParticulate chocolate composition 1.30 as described in Example 3Particulate lemon composition as 1.30 described in Example 2¹⁾spray-dried powder of partially hydrogenated soybean oil, non-fat milkand mono- and diglycerides

Preparation

The ingredients of Part A and Part B were dry blended, an egg as well as600 ml of milk were added to the dry blend and mixed together. The cakemass was then poured in an empty mould. The cake was baked in an oven at190°, until well baked (about 50 min).

The delivery systems were still intact after baking Flavor strength wasstronger than in the control samples prepared directly from thecorresponding chocolate and lemon liquids as iso-loads. In contrary tothe control samples, the flavor profiles were preserved in the bakedapplications. The integrity of the novel delivery systems allowed dualflavor release whereas the taste of the control samples was achocolate-lemon blend.

Example 6 Sugar-Free Hard-Boiled Candy Comprising the ParticulateComposition of the Present Invention

In a copper pan, 100 g of isomalt and 30 g of water are added. The gasframe is turned on and the contents of the copper pan are heated to 165°C. under stirring. Care should be taken as to avoid crystallisation inhard boiled candy. At 165° C., the copper pan is removed from the frameand placed in a water bath at 40° C., and removed after a few seconds.When the temperature has reached 135° C., citric acid (at 0.8 wt. % ofthe candy solution) and liquid flavors (0.5 wt. % of the candy solution)are added.

Meanwhile, particles of the particulate composition obtained in Example2 were added to empty ejector-pins of a TEFLON®-mold. The cooked syrupincluding citric acid and flavors was mixed with a spatula and, at roomtemperature and less than 40% relative humidity, poured intoejector-pins of the TEFLON®-mold comprising the particles. Aftersolidification, the hard-boiled candies are manually ejected from thepins.

In this way, sugar-free hard-boiled candy comprising extruded particlesbased on fiber and comprising lemon flavors were obtained.

Example 7 Gummies Comprising the Particulate Composition of the PresentInvention

Ingredients weight (g) Part A: Gelatine (Bloom no. 250) 240 Water 800Part B: Water 600 Granulated sucrose 1200 Glucose syrup 42 DE (85 brix)1600 Part C: Citric acid 40 Part D: Particle obtained in Example 2 3

800 g water are put in a large PYREX® beaker. Slowly, 240 g of gelatineare added to the water. The gelatine-water solution is mixed untildissolution of all lumps and allowed to swell for 20 minutes. Thereafterit is placed in a water bath (60° C.) until further use (part A).

Separately, a starch tray with a selected impressions (molds) wasprepared.

In a copper pan, 1600 g of glucose syrup 42DE are added, followed by1200 g of granulated sucrose and 600 g of water. The contents of thecopper pan were heated to 112° C. by a gas frame under mixing (part B).Thereafter, the copper pan was placed in a water bath (40° C.) andcooled down to 100° C. by slowly mixing with a spatula. At 100° C., thegelatine solution (part A) is added and mixed well with the a wiremixer. Then, the citric acid (part C) is added and mixed into the cookedsyrup.

In a 500 ml PYREX® beaker, 297 g of the gelatine-cooked syrup (above)and 3 g of the particles of Example 3 (chocolate) are mixed with aspatula and poured into a hot stainless steel depositor and, from there,carefully deposited in each of the empty moulds of the starch tray. Theflavored gelatine-cooked syrup is allowed to dry at 25° C. with lessthan 40% relative humidity for 24 hours. Then, gelatine candies areremoved from the starch tray, placed in a sieve, rinsed with cold water,dried on a perforated stainless steel tray for 4 hours and coated withbee wax to prevent sticking together.

Example 8 Sugar-Free Bubble Gum Comprising the Particulate CompositionWith Tutti Frutti Flavor

Ingredients weight (g) Part A (bubble gum): Mistral-T gum base (CafosaGum Base Co., Spain) 75.24 Crystalline sorbitol powder 159.24 LYCASIN ®75% Maltitol solution 54.18 Glycerine* 10.53 Aspartame 0.24 Total(bubble gum only) 300.00 Part B (Particles of Example 4) 3

Crystalline sorbitol and aspartame are dry blended to form a powder ofblended sweeteners. Half of the sweeteners blend is added to a SIGMA®blade mixer equipped with heated water jacket at temperature about50-55° C. Separately, the gum base is heated for softening, added to theblade mixer and mixed with the powdered sweeteners for 2 minutes. Theremaining powder of blended sweeteners and a humectant syrup (LYCASIN®,Glycerine, Aspartame) is added to the mixer and mixed for at least 7more minutes. The total mixing time was 12 minutes.

The particulate composition comprising a tutti frutti flavor as activeencapsulate ingredient (3 g) was added and mixed to the unflavoredchewing gum base (300 g). The flavored gum was then formed by passingthrough a sheeter machine (Seewer Rondo, Burgdorf, Switzerland), and cutinto the large cubicle shapes typical of bubble gum products.

In this way, a sugar-free, non-cariogenic bubble gum was obtained,comprising the particulate composition of the present invention.

1. A particulate composition in the form of an extruded, glassy bead,comprising a fibrous carrier composition encapsulating an activeingredient, wherein the bead has a cross-section diameter comprisedbetween 3 mm and 15 mm, and the carrier composition comprises from 2 to90% by weight of a first water-soluble fibrous polysaccharide having anaverage molecular weight greater than 10,000 Daltons and an averagedegree of polymerisation greater than 60, and from 1 to 80% of a secondwater-soluble fibrous polysaccharide having an average molecular weightof less than 10,000 Daltons and an average degree of polymerisation ofless than 60, with the percentages being defined by weight relative tothe total weight of the carrier composition.
 2. The particulatecomposition according to claim 1, in which the bead has a cross-sectiondiameter comprised between 5 mm and 15 mm.
 3. The particulatecomposition according to claim 1, in which the carrier composition issugarless or non-cariogenic.
 4. A particulate composition according toclaim 1, wherein the active ingredient is selected from a flavor, afragrance, a vitamin, a drug, a colorant, a nutraceutical, a whiteningagent, an antibacterial agent, and mixtures thereof.
 5. A particulatecomposition according to claim 1, wherein the active ingredient consistsof a flavor ingredient or composition.
 6. A particulate compositionaccording to claim 1, wherein the active ingredient is present in anamount of from 0.01 to 15% by weight relative to the total weight of thecomposition.
 7. A particulate composition according to claim 1, whereinthe first water-soluble fibrous polysaccharide is selected from thegroup consisting of konjac mannan, xanthan, gum Arabic, guar gum,pectin, locust bean gum, soluble soybean polysaccharide and beta-glucanand mixtures thereof.
 8. A particulate composition according to claim 1,wherein the second water-soluble fibrous polysaccharide is a dextrin. 9.A foodstuff or beverage comprising, as part of an edible composition, aparticulate composition according to claim
 3. 10. A foodstuff accordingto claim 9, in the form of a baked product, a hard candy, a gummy candy,a chewy sweet, a chewing gum, a cereal bar, a soup, noodles or a savourysnack.
 11. A foodstuff according to claim 9 in the form of a sphericalhard candy.
 12. A method for the preparation of a particulatecomposition as defined in claim 1, comprising the steps of: a) combiningand blending an ingredient to be encapsulated with a carrier compositioncomprising from 1 to 70% by weight of a first water-soluble fibrouspolysaccharide having an average molecular weight higher than 10,000Daltons and an average degree of polymerisation higher than 60, and from30 to 99% of a second water-soluble fibrous polysaccharide having anaverage molecular weight below 10,000 Daltons and an average degree ofpolymerisation below 60, percentages being given by weight relative tothe total weight of the carrier composition; b) heating said blendwithin a screw extruder to a temperature within the range of from 80° C.to 120° C. to form a molten mass; c) extruding the molten mass through adie having a die hole diameter comprised between 4 and 12 mm; and d)cutting the material obtained as it exits the die.